Two different radiochemical procedures were developed: chelate ion resin exchange and amine solvent extraction. Two kinds of new Chinese chelate resins (NANKAI-3926 and BEI-5) and a new longchain primary amine N1923 were compared with the Srafion NMRR and the tertiary amine N235 in absorption performance of noble metals, respectively. Influences of various experimental conditions, e. g. sample digestion, acidity, equilibrium time, as well as elution of noble metals, on analytical sensitivity and chemical yield were discussed. Combining with neutron activation, the radiochemical separation procedures developed were used to determine the noble metal contents in the geological samples from Permian/Triassic boundary in South China.